With the aim to improve the purity of total flavonoids of Cyclocarya paliurus leaves, the suitable resin for separating and purifying total flavonoids of Cyclocarya paliurus leaves and the optimum parameters of purification were studied. The optimal techniques of separation and purification of flavonoid were obtained by static adsorption and elution tests, and the separation techniques were evaluated by measuring the concentration of total flavonoids of Cyclocarya paliurus leaves with ultraviolet spectrophotometer. The results showed that the AB—8 macroporous resin gave the best effect of separation with the sampling rate 2BV/h and concentration 1.0mg/mL, respectively, and the concentration of elution was 70% alcohol, with eluting velocity 2BV/h. In conclusion, AB—8 resin could be applied to purify total flavonoids of Cyclocarya paliurus leaves.